CN108654668A - A kind of thin layer g-C3N4Preparation method - Google Patents
A kind of thin layer g-C3N4Preparation method Download PDFInfo
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- CN108654668A CN108654668A CN201810377550.3A CN201810377550A CN108654668A CN 108654668 A CN108654668 A CN 108654668A CN 201810377550 A CN201810377550 A CN 201810377550A CN 108654668 A CN108654668 A CN 108654668A
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- 238000000034 method Methods 0.000 title abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000007787 solid Substances 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002604 ultrasonography Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 7
- 239000010410 layer Substances 0.000 description 22
- 239000002585 base Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229920002620 polyvinyl fluoride Polymers 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ZIPLUEXSCPLCEI-UHFFFAOYSA-N cyanamide group Chemical group C(#N)[NH-] ZIPLUEXSCPLCEI-UHFFFAOYSA-N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
Abstract
The present invention relates to a kind of thin layer g C3N4Preparation method, it includes the following steps:(a) it is calcined at a temperature of nitrogenous precursor being placed in 400~650 DEG C, grinds to obtain solid powder;(b) solid powder, alkali piece and water are added into container, is transferred in reaction kettle, is reacted at a temperature of being placed in 80~150 DEG C, centrifuging and taking filter residue after ultrasound;The alkali piece is NaOH or KOH;(c) filter residue and water are added into another container, is transferred in reaction kettle, is reacted at a temperature of being placed in 80~150 DEG C, centrifuging and taking filter residue is freeze-dried after ultrasound.The thin layer g C that surface area is high, pattern is single can be obtained in this way3N4;And this method hydrothermal temperature is low, it is short to take, and effective approach is provided for photochemical catalyst.
Description
Technical field
The invention belongs to catalyst fields, are related to a kind of photochemical catalyst, and in particular to a kind of thin layer g-C3N4Preparation side
Method.
Background technology
Sentence talk about " the furthest distance in the world it is not raw with it is dead, I leads your hand at Beijing crossing and but sees
Less than your face ", the use of fossil energy not only brings the convenient prosperity with life to us, following also environment
Pollution, and fossil energy belongs to the not renewable sources of energy, us is thus forced to seek the more clean energy.
Combustion of hydrogen releases a large amount of energy, and water, cleanliness without any pollution are generated after burning.The mode of production hydrogen mainly has at present
Three kinds, respectively:The recombination of fossil energy regenerates, electro-catalysis and photocatalysis.But the recombination of fossil energy regeneration still can produce
Raw CO2Equal gases do not solve air problem, and electro-catalysis can consume a large amount of energy, and photocatalysis is due to being to utilize sunlight
And it attracts attention.Efficiency of selection is high, low energy consumption, and photochemical catalyst simple to operate then becomes people's urgent problem to be solved.
Since the electrode decomposing potential of water is 1.23eV, simultaneously because the presence of overpotential, the position of energy band of photochemical catalyst
It should be greater than 1.8eV or more.g-C3N4It is the structure of a type graphite, is combined between layers with the effect of molecular force.In recent years
g-C3N4Since it belongs to nonmetallic materials, energy gap is relatively low (2.7eV), can absorb the sunlight spectrum of wider range,
And due to g-C3N4There is different degrees of defect on surface, which can be as the trap center of electrons and holes, to make electronics
Compound the advantages that abundant active site is provided simultaneously is not easy to after being detached with hole and rather well received.
g-C3N4It is generally synthesized by heating polycondensation by cyanamide, melamine etc., as shown in Figure 1;But heating condensation polymerization
At mostly be bulk g-C3N4(accumulate g-C3N4), the g-C of body phase3N4It is the g-C by single layer3N4It accumulates, due to
Its is intermolecular to cause its surface area relatively low there are more serious sedimentation, only about 10m2/g;In fully decentralized state
The g-C of lower single layer3N4Specific surface area be up to 2500m2/ g, it is clear that by bulk g-C3N4Stripping is the state tool of single layer or thin layer
There is the meaning of reality.Current lift-off technology mainly has ultrasound stripping, the stripping of alkali metal ion intercalation and soda acid etching stripping
The methods of, these method and steps are complicated, condition is harsh and cause with high costs.
Invention content
A kind of utilization thin layer g-C is provided the invention aims to overcome the deficiencies in the prior art3N4Preparation method.
In order to achieve the above objectives, the technical solution adopted by the present invention is:A kind of thin layer g-C3N4Preparation method, it includes
Following steps:
(a) it is calcined at a temperature of nitrogenous precursor being placed in 400~650 DEG C, grinds to obtain solid powder;
(b) solid powder, alkali piece and water are added into container, is transferred in reaction kettle after ultrasound, is placed in 80~120
It is reacted at a temperature of DEG C, centrifuging and taking filter residue;The alkali piece is NaOH or KOH;
(c) filter residue and water are added into another container, is transferred in reaction kettle after ultrasound, is placed in 160~300 DEG C
At a temperature of reacted, centrifuging and taking filter residue is freeze-dried.
Optimally, in step (a), the nitrogenous precursor is selected from cyanamide, dicyandiamide, melamine, thiocarbamide and urea
The mixture of one or more compositions in element.
Optimally, in step (b), the mass ratio of the solid powder and the NaOH are 4~5:1.
Optimally, in step (b), residue washing to neutrality is then dried in vacuo.
Optimally, it in step (c), will be freeze-dried after residue washing to neutrality.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art:Thin layer g-C of the present invention3N4
Preparation method, by the way that the solid powder of nitrogenous precursor calcining gained is first pre-processed with alkali piece, then using hydro-thermal method
It is removed, the thin layer g-C that surface area is high, pattern is single can be obtained in this way3N4;And this method hydrothermal temperature is low, time-consuming
It is short, provide effective approach for photochemical catalyst.
Description of the drawings
Fig. 1 is that existing heating polycondensation synthesizes g-C3N4Flow chart;
Fig. 2 is the SEM figures of yellow solid in embodiment 1;
Fig. 3 is the SEM figures of step (b) product in embodiment 1;
Fig. 4 is thin layer g-C in embodiment 13N4SEM figure.
Fig. 5 is thin layer g-C in embodiment 13N4With bulk g-C3N4Catalytic performance comparison diagram.
Specific implementation mode
Thin layer g-C of the present invention3N4Preparation method, it includes the following steps:(a) nitrogenous precursor is placed in 400~650
It is calcined at a temperature of DEG C, grinds to obtain solid powder;(b) solid powder, alkali piece and water are added into container, after ultrasonic
It is transferred in reaction kettle, is reacted at a temperature of being placed in 80~120 DEG C, centrifuging and taking filter residue;The alkali piece is NaOH or KOH;
(c) be added the filter residue and water into another container, be transferred in reaction kettle after ultrasound, at a temperature of being placed in 160~300 DEG C into
Row reaction, centrifuging and taking filter residue are freeze-dried.Solid powder elder generation as obtained by calcining nitrogenous precursor and alkali piece
It is pre-processed, then is removed using hydro-thermal method, the thin layer g-C that surface area is high, pattern is single can be obtained in this way3N4;And
This method hydrothermal temperature is low, it is short to take, and effective approach is provided for photochemical catalyst.
Above-mentioned nitrogenous precursor is one or more groups in cyanamide, dicyandiamide, melamine, thiocarbamide and urea element
At mixture.In step (b), the mass ratio of the solid powder and the NaOH are 4~5:1.In step (b), by filter residue
Washing is then dried in vacuo to neutrality.In step (c), it will be freeze-dried after residue washing to neutrality.
Below in conjunction with embodiment, invention is further explained.
Embodiment 1
The present embodiment provides a kind of thin layer g-C3N4Preparation method, it includes the following steps:
(a) poly cyanamid is put into the crucible of wash clean, is then put into (together with crucible) in Muffle furnace and carries out 550 DEG C of calcinings
3 hours (calcining in air, heating rate and rate of temperature fall are 3 DEG C/min);It is cooled to room temperature rear crucible, is ground with agate
Alms bowl is fully ground, and obtained yellow solid (is bulk g-C3N4), the SEM figures of yellow solid are as shown in Figure 2;
(b) it is separately added into 0.5g yellow solids and 0.12gNaOH into the polyvinyl fluoride bottle of 50mL, 30mL deionizations are added
Water is transferred in the reaction kettle of 50mL after ultrasonic 30min, is subsequently placed into baking oven and is heated 20h (temperature is 100 DEG C);It is to be heated
After, it is centrifuged and sample (i.e. filter residue) is washed with deionized to neutrality, then do sample progress vacuum
Dry (vacuum drying temperature is 40 DEG C), the sample (SEM figures are as shown in Figure 3) after drying are ground;
(c) product of 0.1g steps (b) is added into the polyvinyl fluoride bottle of 50mL, 30mL deionized waters, ultrasound is added
It is transferred in the reaction kettle of 50mL after 30min, is subsequently placed into baking oven and heats 6h (temperature is 200 DEG C);After to be heated, into
Row centrifuges and sample (i.e. filter residue) is washed with deionized to neutrality, then carries out the sample (SEM schemes as shown in Figure 4)
Freeze-drying.Bulk g-C as can be seen from Figure 23N4Surface is more coarse, and presentation is blocky and thicker, therefore can influence
Extinction causes performance bad;Fig. 3 schemes for pretreated SEM, and pattern has no too big difference with before pretreatment;Fig. 4 is
G-C after being removed3N4SEM figure, the g-C after as can be seen from the figure being removed3N4Surface roughness becomes smaller, and is thin
Layer compares bulk g-C3N4Specific surface area obviously greatly, therefore to participate in that light-catalysed area is also bigger, and performance is just also better;
Fig. 5 is catalytic performance comparison diagram, it is known from figures that bulk g-C3N4H2-producing capacity be 280 μm of ol/g/h, after stripping
g-C3N4For 750 μm of ol/g/h.G-C after stripping3N4Obviously than bulk g-C3N4Nearly three times are higher by, this is because after stripping
g-C3N4Photo absorption performance enhances, and participates in the increased reason of specific surface area of production hydrogen, matches with the SEM of the foregoing description.
Embodiment 2
The present embodiment provides a kind of thin layer g-C3N4Preparation method, it with it is almost the same in embodiment 1, unlike:
In step (b), the temperature of baking oven is 80 DEG C;In step (c), the temperature of baking oven is 160 DEG C.
Embodiment 3
The present embodiment provides a kind of thin layer g-C3N4Preparation method, it with it is almost the same in embodiment 1, unlike:
In step (b), the temperature of baking oven is 120 DEG C;In step (c), the temperature of baking oven is 300 DEG C.
Embodiment 4
The present embodiment provides a kind of thin layer g-C3N4Preparation method, it with it is almost the same in embodiment 1, unlike:
In step (b), the mass ratio of yellow solid and NaOH are 4:1.
Embodiment 5
The present embodiment provides a kind of thin layer g-C3N4Preparation method, it with it is almost the same in embodiment 1, unlike:
In step (b), the mass ratio of yellow solid and NaOH are 5:1.
Comparative example 1
The present embodiment provides a kind of thin layer g-C3N4Preparation method, it with it is almost the same in embodiment 1, unlike,
Step (b) is not carried out.
Comparative example 2
The present embodiment provides a kind of thin layer g-C3N4Preparation method, it with it is almost the same in embodiment 1, unlike:
In step (b), NaOH 0.5g are excessive.
It is mainly that temperature is different, and temperature is than in embodiment 1 in embodiment 2 in embodiment 1, embodiment 2 and embodiment 3
Low, temperature is relatively low to cause pretreatment to be not enough with stripping, cause the specific area of g-C3N4 relatively low, light-catalysed to make
Activity reduces;And temperature drift can cause the structure of g-C3N4 that it is bad to also result in photocatalysis performance by destruction.Embodiment
1, it is mainly that base amount is different, and the base amount in embodiment 4 is than big in embodiment 1, alkali in embodiment 4 and embodiment 5
Dosage can excessively cause g-C3N4 to be destroyed to the structure of g-C3N4 in stripping, therefore can also influence light-catalysed performance.
Base amount in embodiment 5 is on the low side, and the reduction of base amount can lead to g-C3N4It removes not complete enough, participates in the area meeting of reaction
It reduces, to which photocatalysis performance is bad.It is not pre-processed in comparative example 1, leads to g-C3N4Molecular force between layers compared with
Greatly, must almost arrive thin layer g-C3N4;Base amount in comparative example 2 is excessive, destroys g-C3N4Structure, lead to photocatalysis
Performance drastically decline and requirement be not achieved.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of thin layer g-C3N4Preparation method, which is characterized in that it includes the following steps:
(a) it is calcined at a temperature of nitrogenous precursor being placed in 400~650 DEG C, grinds to obtain solid powder;
(b) solid powder, alkali piece and water are added into container, is transferred in reaction kettle after ultrasound, is placed in 80~120 DEG C
At a temperature of reacted, centrifuging and taking filter residue;The alkali piece is NaOH or KOH;
(c) filter residue and water are added into another container, is transferred in reaction kettle after ultrasound, is placed in 160~300 DEG C of temperature
Under reacted, centrifuging and taking filter residue is freeze-dried.
2. the preparation method of thin layer g-C3N4 according to claim 1, it is characterised in that:In step (a), it is described it is nitrogenous before
Drive the mixture that body is one or more compositions in cyanamide, dicyandiamide, melamine, thiocarbamide and urea element.
3. the preparation method of thin layer g-C3N4 according to claim 1, it is characterised in that:In step (b), the solid powder
The mass ratio of the last and described NaOH is 4~5:1.
4. the preparation method of thin layer g-C3N4 according to claim 1, it is characterised in that:In step (b), by residue washing
To neutrality, then it is dried in vacuo.
5. the preparation method of thin layer g-C3N4 according to claim 1, it is characterised in that:In step (c), by residue washing
It is freeze-dried after to neutrality.
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CN110980665A (en) * | 2019-11-29 | 2020-04-10 | 平顶山学院 | Preparation method of two-dimensional thin-layer structure carbon nitride |
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CN104944392A (en) * | 2014-03-25 | 2015-09-30 | 中国科学院大连化学物理研究所 | Mass preparation method of graphite-phase carbon nitride nanosheets |
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CN104944392A (en) * | 2014-03-25 | 2015-09-30 | 中国科学院大连化学物理研究所 | Mass preparation method of graphite-phase carbon nitride nanosheets |
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